Patent GB-711406-A (GB)
Title: Process for the catalytic hydrogenation of carbon monoxide
IPC: B01J23/745
Filed: 1952-04-10
Abstract: Hydrogenation of carbon monoxide is carried out in the presence of an iron catalyst prepared by precipitating a solution of iron sulphate in such a manner that about 10-50 per cent of the iron in the precipitate is in trivalent form, washing the precipitate with an aqueous solution of ammonia, an ammonium compound, or an aliphatic amine, and then drying, the precipitate being treated with a gaseous oxidizing medium during washing and drying so that more than 70 per cent of the iron is in the trivalent form on completion of drying (see Group III).  When a high synthesis yield of oxygen-containing compounds, particularly alcohols, is required, the catalyst contains at least 50 per cent of the iron in the free state, and is impregnated before drying with an alkali; when hydrocarbons are required, the catalyst has less than 50 per cent of the iron in the free state, and is impregnated with an alkali metal salt of boric, phosphoric, silicic, or tungstic acids.  Synthesis may be a single-stage or multi-stage process, with or without gas recycling and removal of carbon monoxide between the stages; the temperature may be 150-300 DEG  C. and the pressure 1-100 atmospheres.  Gas containing from 0.5-2 or more volumes of hydrogen per volume of carbon monoxide is passed through a bed of catalyst of depth 5-12 metres or more at a rate of 10-500 volumes or more per volume of catalyst per hour.ALSO:An iron catalyst for the hydrogenation of carbon monoxide (see Group IV (b)) is prepared by precipitating a solution of iron sulphate in such a manner that about 10-50 per cent. of the iron in the precipitate is in the trivalent form, washing the precipitate with an aqueous solution of ammonia, an ammonium compound, or an aliphatic amine, and then drying, the precipitate being treated with a gaseous oxidising medium during washing and drying so that more than 70 per cent. of the iron is in the trivalent form on completion of drying.  A solution of ferrous sulphate, which may also contain silver, copper, or calcium, is added to a solution of an alkali metal hydroxide, carbonate, or bicarbonate at 50-100 DEG C., and heated air is bubbled through the mixed solutions; the precipitate is filtered off, washed with water and then with a solution of ammonium nitrate, carbonate, or acetate until free from sulphate ions, and finally dried in a stream of air at 100 DEG -110 DEG C.  Reduction may be effected in the synthesis reactor at 150 DEG -350 DEG C. by the passage of hydrogen or carbon monoxide, with or without nitrogen, at a speed greater than 1 meter/second, the catalyst being in layers of 30-100 cms. or greater.  Carriers such as alumina or silicons materials may be included in the catalyst.  When a high synthesis yield of oxygen-containing compounds is required, the catalyst contains at least 50 per cent. of the iron in the free state, and is impregnated before drying with 2-15 per cent. of alkali based on the iron content; when hydrocarbons are required, the catalyst has less than 50 per cent. of the iron is the free state, and is impregnated with an alkali metal salt of boric, phosphoric, silicic or tungstic acids, the acid content being greater than 1 per cent. and the alkali content from 1-10 per cent., based on the iron present.